Preparation method of alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin

A technology of exchange resin and manufacturing method, which is applied in the direction of anion exchange, ion exchange, chemical instruments and methods, etc., can solve the problems of high manufacturing cost of anion exchange resin products, unsuccinct and efficient treatment process, etc., and achieve convenient amination React, improve product appearance, and realize the effect of timely recycling

Active Publication Date: 2018-05-29
雷引林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

That is to say, the manufacturing cost of the whole anion exchange resin product remains high due to the inconvenient and efficient solvent post-treatment process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First according to Chinese invention patent application (application number: 201110083107.3) embodiment 1-3 corresponding test condition and method described in No. 8 test, coordination polymerization prepares linear poly(styrene-ethylene) alternating copolymer, uses GPC Measured by the method (using polystyrene as the standard sample, mobile phase is 1,2-C 6 D. 4 Cl 2 , the temperature is 145°C): M n 42,000, molecular weight distribution coefficient (M w / M n ) is 2.07, use 1 HNMR method records (solvent is C 2 D. 2 Cl 4 , the temperature is 120°C, PS mol%=4A ar / (5A al +A ar ), where A ar Represents the number of protons in the benzene ring of the polystyrene component, A al Represents the number of protons in the aliphatic chain (including the ethylene of the polyethylene component and the polystyrene component): the content of the polystyrene component is 47mol% (mole percent), which is converted into a mass content of 76.7% (equal to 104.15 ×47 / (104.15...

Embodiment 2

[0022] In the fifth step of the "preparation steps of alcohol-soluble anion exchange resin" of Example 1, "add 1.2L (about 1100g, containing about 330g of trimethylamine) with a content of about 30% trimethylamine aqueous solution, 6.8L of deionized water , evacuate and condense at 36-40°C for 10 hours", replace it with "add 600mL (about 530g) of dimethylethanolamine, 7L of deionized water, and evacuate and condense at 40-43°C for 12 hours", the rest of the raw materials and formula With the same operating conditions, about 710g of light yellow quaternary ammonium anion exchange resin product was obtained.

[0023] Referring to the conventional strong basic ion exchange resin test method, the measured anion exchange capacity is 2.54mmol / g dry material, and the water absorption rate is 180%. Further determination of solubility in alcohol (35°C) was: 6.8g / 100mL in methanol, 11.4g / 100mL in ethanol, 21.1g / 100mL in isopropanol, and 19.3g / 100mL in n-butanol.

Embodiment 3

[0025] In the fifth step of the "preparation steps of alcohol-soluble anion exchange resin" of Example 1, "add 1.2L (about 1100g, containing about 330g of trimethylamine) with a content of about 30% trimethylamine aqueous solution, 6.8L of deionized water , evacuated condensation reaction at 36-40°C for 10 hours", use "add 1L (about 750g) of dimethyl n-butylamine, 500mL of acetone, 5.5L deionized water, and ventilated condensation reaction at 45-50°C for 15 hours" Instead, all the other raw materials, formulations and operating conditions were unchanged, and about 700g of light yellow quaternary ammonium anion exchange resin product was obtained.

[0026] Referring to the conventional strong basic ion exchange resin test method, the measured anion exchange capacity is 2.43mmol / g dry material, and the water absorption rate is 160%. Further determination of solubility in alcohol (35°C) was: 6.6g / 100mL in methanol, 9.3g / 100mL in ethanol, 18.9g / 100mL in isopropanol, and 17.2g / 100mL ...

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Abstract

The invention discloses a preparation method of alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin. The preparation method of the alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin comprises the following steps: taking a linear poly(styrene-ethylene) alternating copolymer as a raw material, completely dissolving the linear poly(styrene-ethylene) alternating copolymer into halogenated hydrocarbon, then adding an industrial chloromethyl ether solution dissolved with a catalyst, and carrying out homogeneous-phase chloromethylation reaction; then enabling a reaction product to pass through a stainless steel high-pressure nozzle; extruding the reaction product into water which contains a dispersing agent and sodium hydroxide; rapidlydispersing into a suspension system by using a stirring paddle with a cutting function; carrying out reduced pressure distillation to recycle the halogenated hydrocarbon; after filtering and drying the suspension particles, washing the suspension particles with water thoroughly, and adding an organic amines aqueous solution to react; filtering and drying residual reaction liquid, adding diluted hydrochloric acid to neutralize, filtering and drying, and then washing for multiple times by using deionized water; and finally filtering and drying, and blowing and drying the solid particles to obtain an alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin product. Quaternary amine or tertiary amine groups in the product prepared by the method are distributed uniformly, and can be completely dissolved in low-toxicity organic alcohol.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, in particular to a poly(styrene-ethylene) alternating copolymer, which can be completely dissolved in alcohol organic solvents, and has strong basic quaternary amino groups or weak basic tertiary amino groups. A functional resin material with amino functional groups capable of undergoing anion exchange and a manufacturing method thereof. Background technique [0002] Linear polymer materials containing quaternary or tertiary aminated polystyrene components (also known as aminated polystyrene-based polymers), due to their ability to be highly swellable in water and moderately soluble in organic solvents , Strong hydrophilicity, anion exchange and other physical and chemical properties, are widely used in various fields such as hydrophilic membrane preparation, water treatment, energy and so on. For example, as the main material or auxiliary additive material of positively charged membr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J41/14C08F212/08C08F210/02C08F8/32C08F8/44C08F8/24
CPCB01J41/14C08F8/32C08F8/44C08F8/24C08F212/08
Inventor 雷引林高章华陈飞李南文廖家友殷锦邓承毅
Owner 雷引林
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